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Method for reversible chain transfer catalytic polymerization of polymerization system under phosphine catalysis

A catalytic polymerization and chain transfer technology, which is applied in the field of reversible chain transfer catalytic polymerization, can solve the problems of polymer performance impact, crosslinking, and wide molecular weight distribution index of polymers, and achieve the effect of efficient synthesis and convenient acquisition

Inactive Publication Date: 2013-08-14
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the nature of free radical polymerization determines that the polymerization reaction is difficult to control, which leads to a wide molecular weight distribution index of the polymer, uncontrollable molecular weight and structure, and often occurs disproportionation, crosslinking, etc., which greatly affects the performance of the polymer.

Method used

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  • Method for reversible chain transfer catalytic polymerization of polymerization system under phosphine catalysis
  • Method for reversible chain transfer catalytic polymerization of polymerization system under phosphine catalysis
  • Method for reversible chain transfer catalytic polymerization of polymerization system under phosphine catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step 1) Synthesis of iodoisobutyronitrile

[0039] see figure 1 As shown, weigh 25.0 mmol of azobisisobutyronitrile, measure about 50 mL of benzene and place it in a three-necked flask, and protect it with argon; weigh 50.4 mmol of iodine, add it to the above solution, and then add about 30 mL of benzene; Heat to 90 °C and reflux for 6-8 h; remove the reaction and cool to room temperature, add about 80 mL of saturated Na 2 S 2 o 3 solution, stirred until the color faded to light yellow; separatory funnel liquid separation, the lower liquid (aqueous solution) was discarded, and the upper layer (organic layer) was washed with saturated Na 2 S 2 o 3The solution (40 mL×2) was washed twice, and the upper layer (organic layer) was poured into the Erlenmeyer flask (the outer side of the Erlenmeyer flask was wrapped with aluminum foil), and about 15 scoops of anhydrous Na 2 SO 4 , placed on top of the refrigerator to dry overnight. Post-processing (vacuum distillation)...

Embodiment 2

[0053] Embodiment 2: Different iodine reagents take triphenylphosphine as a catalyst to prepare polymer PSt by reversible chain transfer catalytic polymerization

[0054] The difference with Example 1 is: the reaction ratio is [styrene] 0 : [Iodoisobutyronitrile] 0 : [Dicumyl Peroxide] 0 :[Triphenylphosphine] 0 = 100:0.1-1:0.1-1:0.1, the polymer PSt was obtained by reaction, and the results are shown in Table 2.

[0055] In Table 2, St is styrene, CPI is iodoisobutyronitrile, DCP is dicumyl peroxide, and TPP is triphenylphosphine, M n,th For the theoretically calculated molecular weight, M n,GPC and M w / M n Polymer molecular weight and molecular weight distribution determined for gel chromatography. GPC is gel chromatography. The data in row 1-4 in Table 2 is [styrene] 0 : [Dicumyl Peroxide] 0 =100: the polymerization result at 0.1-1; the data in rows 5-7 in Table 2 are the polymerization results of different amounts of iodoisobutyronitrile and different amou...

Embodiment 3

[0059] Example 3: Preparation of Polymer PSt by Reversible Chain Transfer Catalytic Polymerization under Different Phosphine Catalysts

[0060] The difference with Example 1 is: the reaction ratio is [styrene] 0 : [Iodoisobutyronitrile] 0 : [Dicumyl Peroxide] 0 : [P-Cata] 0 = 100:0.1-1:0.1-1:0.1, P-Cata in order: triphenylphosphine TPPO, TBPBr, CH 2 P 2 Ph 4 , C 2 h 4 P 2 Ph 4 One of them, the reaction yields polymer PSt with controllable activity.

[0061] In Table 3, TPPO is triphenylphosphine oxide, TBPBr is tetra-n-butylphosphine bromide, CH 2 P 2 Ph 4 is bis(diphenylphosphine)methane, C 2 h 4 P 2 Ph 4 is 1,2-bis(diphenylphosphine)ethane, M n,th For the theoretically calculated molecular weight, M n,GPC and M w / M n Polymer molecular weight and molecular weight distribution determined for gel chromatography. GPC is gel chromatography, and the data in rows 1-4 are the polymerization results of different phosphine catalysts. The results show that...

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Abstract

The invention discloses a method for reversible chain transfer catalytic polymerization of a polymerization system under phosphine catalysis. The method comprises the following steps of: preparing the polymerization system, and carrying out reversible chain transfer catalytic polymerization reaction for 0.5-24 hours at 40-110 DEG C; carrying out separation and purification to obtain a polymer; carrying out nuclear magnetic resonance on the polymer; and carrying out gel chromatograph structural analysis. Compared with the catalyst adopted in the past, the polymerization system is simple and efficient and is convenient and easy to obtain, a method and a means for application of catalytic initiating systems of the type in polymer synthesis are provided, the theoretical preparation for efficiently and quickly preparing polymers with various functions is provided, and a practical general plan for more conveniently, simply and efficiently synthesizing functional polymer materials in an environment-friendly way is provided.

Description

technical field [0001] The invention relates to a reversible chain transfer catalytic polymerization method using a novel catalyst, in particular to a reversible chain transfer catalytic polymerization method for a polymerization system under phosphine catalysis. Background technique [0002] Since Szwarc proposed the concept of living polymerization, a variety of living polymerization methods, such as anionic polymerization, cationic polymerization, ring-opening polymerization, complex anionic polymerization and metal-free anionic polymerization, have been discovered and reported one after another. Although these living polymerizations can prepare polymers with controllable structures, the relatively harsh reaction conditions limit their development, especially ionic polymerization has very strict requirements on the polymerization conditions: the purity of the reaction system is high, and there should be no trace impurities (such as water , carbon dioxide and other acidic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F120/14C08F4/04C08F4/34C08F2/02C08F2/06
Inventor 程振平柏良久龚学锋张丽芬朱秀林朱健张正彪周年琛张伟
Owner SUZHOU UNIV
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